Method for producing carbon bisulphide



July 8, 1941. so s 2248509 METHOD FOR PRODUCING CARBON BISULPHIDE Filed Jan. 31, 1939 %Tom Patented July 8, 1941 ICE METHOD FOR PRODUCENG CARBON V BISULPHIDE Frank' H..ParsonsFairpo-t Harbor, Ohio, assignor of: one -fourth to William Ahlstrom, Mentor, h.io,- one-fourth to John A. Horacek, and oneforthsto Richard J. Tischler, both of Fairport Harbor; Ohio Application January 31, 1939, Serial No. %3,823 6oClaims. -(Cl.' 23-206) This invention rel'ates to a method and apparatus for producing chem'cal reactions, and' is particularly appli'cable to reactions which must take place while the materialsinvolved are'- subjected to relatively high temperatures;

An' object of the nvention is to providearrimproved' method which may be easily'performed.

Another.. object of the invention is to provide an improved method which will: be consistent in operation;

Another object. of; the i'nvention is to" provide an improved methodwhich will: produce a' product free from uncombined.material`s;.

Another object' of' the `invention: iss-to provide an: improved method which: will he therrnally eihcient;

Another object of" the invention is' to: provide an improved method by' which carbon bi: sulphlde may be easily and economically' produced.

Another' object: isto provid'e 'an improved apparatus inwhich' the quantities` of uncombined constituents'present in the: apparatus are small in 'relation to::` output:

Another' object is: to: provide ani improved apparatus in* whioh the-` control of temperature, pressure, and input of rawmaterials; are stable and easily controlled Another` object is to provide: 'an' improved apparatus which may" bmrapidly cooled:

Another object is to -provide an improved ap'- paratus which willpro'vide easy access for inspection, replacement, and repair.

Another object isto provide an improved* apparatus in which: the solidication of raw materials caused by taking the equipment' out of serviceisof nohindrance tothe resumption of operation? or the internal inspeotion-` of the apparatus: r

Another: objectis to providean improved ap paratus in= which: relatively: little energy is required: for heating purposes;

Another object is to provide an improved ap paratus which. will effectively 'separate gaseous materials;

Anotherob-jec t:- lsto provide an improved: ap paratuswhich will be` simple` in Construction.

Another object isto provide-an improved ap paratus which may be: easily and economically operated. e i

Another object is to providean paratus whichwilLoccpy small space relative to its output.

Another object is: to.-provide-a n improved apparatus which :is more efii i nt bythe re l sma tiono waste-heat:

improved' apv 'Other objects will hereinafter appear.

The invention will be better understood` from the description of one practical embodiment of the apparatus, and the method which may be performed by use of this apparatus, illustrated in the'accompanying drawing, in which:

Figure 1 is a central sectional view of the apparatus arranged in a convenient manner for the production of c'arbon bi-sulphide (CS2)'; i

Figura 2' is a transverse sectional view taken on the line'II-II of Figure 1; 'and' r Figure 3 is a transverse sectional view taken on line III- III of' Figure 1.

The' device consists of a lower vaporizirigand re'action" chamber portion and' an upper' separatin'g portion indicated generally by A and B, respectively. The Vaporizing and'reaction cham ber comprises a floor or base I of heatinsulating material, such as fire brick or other refractory substance. Upon this base are built four walls, 2; 3, 4; and' 5; forming a generally rectangular chamber, the walls also being composed of' refractory material, and shown as protected'by an outermetallic shell or casing 6.

Adjacent the wall 4', 'and parallel thereto, is a bame' wall 'l, terminating somewhat below the top of walls 2, 3, 4; and 5 and being provided' in its lower portion with an 'aperture 8.' In this aperture is .positioned a fan or propeller &mounted on' a shaft lil driven from the exterior of the device by any suitable'driving means; suchasan electric motor (not shown).

Extending across the space define'd by w'alls 2; 3; 1, and 5, is a' grid composed of horizontal bars ll of electric conducting material having sufiiciently high resistance to serve as a heating element.

These'bars are compo'sed of a' material' which will not introduce undesired constituents into the chamber, and which has sufciently high refractory characeristics to withstand th'e' temperatures maintained therein. The 'bars are electrically connected in series, as shown' in Figure 3,- andther ends project' through wall 5'for connection to any suitable source of current. A material which we have found' particularly suitable for' this purpose when used-in the production of carbon bi-sulphide is carborundum; which may be readily fo-rmed into a grid asindi'cated; and efliciently transformselectrical energy into heat, -as required in this process, while possessing the' necessary strength torenderit particularly suitable for this purpose;

Control of the heat maybe Secured by; any desired or well known ty e of electrical control".

Beneath the grid, a Conduit !2 extends horizontally through the wall 2, having its outer end connected with a jacketed tank !3, the jacket of which s indicated at !4, in which tank material such as the sulphur required in the production of CS2 may be melted and through which Conduit it may be conducted to a reservoir formed by the lower edges of walls 2, 3, and and base l, this reservoir being quite shallow and terminating beneath the pipe !2 and orifice 8. 1

Through the wall 2, above the grid, extends another conduit !5, through which solid material, such as charcoal, may be fed to the upper surface of the grid.

Both conduits !2 and !5 may very Conveniently be made of carborundum which will not be deleteriously afiected by heat within the apparatus.

connected to the conduit !5 is a stoker !6, arranged to remove solid material from a hopper or bin !1 and to feed it into the space above the grid as required.

Resting upon the top of walls 2, 3, 4, and 5, is the Separator B, consistng of an outer oylindrical shell !8, upper and lower heads !9 and 29, respectively, and a plurality of vertical tubes 2! seaied to the two heads. Upon the upper head !9 is secured a frustro-conical cap 22 having its upper end flanged, as indicated at 23, for connection to a conduit or the like for conducting away the products of the apparatus.

Pipes 24 connect the space within the separator shell to the space within the jacket !4 and also to any other apparatus to which it is desired to furnish steam, while a pipe 25 is coni nected to a source of water for supplying the space within the Separator.

The operation of the device in producing carbon bisulphide is as follows:

charcoal is fed from the bin !1 by means of the stoker !6 and drops from tube !5 into a pile C, resting upon the top of grid bars sulphur is placed in the tank !3 where it is melted by steam in the jacket !4, so that it may flow from the tank through the pipe !2 to the reservoir in the interior of the apparatus. Its flow is controlled by a valve V. Initially the valve V is closed, the motor driving fan 9 is started and this circulates the atmosphere in the directions indicated by the arrows, drawing it downwardly and propelling it through the oriflce 8 under the grid.

During the starting up of the apparatus, electric current is supplied to grid bars which thus are heated to initiat-e combustion by which the oxygen is consumed, and thereafter raises the temperature of the grid bars to somewhat above the lowest point at which the carbon and sulphur can directly combine, or, in other words, the minimum formaticn temperature of carbon 'bisulphide (approximately 1472 F.)

This circulation of the atmosphere is continued until ali oxygen in the apparatus has been con- 'sumed by combustion of some of the charcoal and converted into carbon doxide. 'oxygen has thus been consumed, the valve V is opened, permitting sulphur to flow through the pipe !2 to form a pool S in the bottom of the reservoir.

The currents induced in the atmosphere by fan 9 force the same between the grid bars and through the charcoal or carbon piled upon these bars repeatedly, the atmosphere beccming highly heated, and in blowing across the pool S, asssist ing the downwardly directed radiant heat in the When all the grid bars in vaporizing the molten sulphur in this pool.

As soon as this atmosphere has reached the Iori remains in gaseous condition and passes through these tubes, the sulphur returning to liquid form and running down the tubes, dripping from the bottom 'ends' thereof to be picked up by the hot gases in thereaction chamber, revaporized, and carried around through the charcoal pile until' italso has combined with carbon.

Of course, charcoal and sulphur are supplied by the stoker !6 and tank !3, respectively, to replace these materials, as they are consumed and thus, at'all times, to maintain the necessary quantities of the materials.

Thus, it will be seen that all uncombned sulphur vapor ,is circulated through the charcoal, again and again, as many times as may be necessary to cause it fully to enter into combination, and that each time, as it approaches the charcoal, it passes through the heated grid bars so that it reaches the charcoal at a temperature suitable for combination therewith. i

It will be understood that "circulating" as used herein implies 'passing the material through a closed path a plurality of times, as diiferentiated from passing along an open path by which it would have an'opportunity to contact th solid material only once. x

Rapid combination is effected, both because of the circulation' and'heating' of the sulphur vapor and because of the arrangement which causes this vapor to effectively penetrate through all the intricacies of the pile of charcoal.

i Heat' given off by the sulphur as it condenses in the Separator, of course, is transmitted to the water in this Separator, converting the same into steam, part of which 'is shown as used for melting the sulphur being supplied, and part as being conducted away' for use by other apparatus, so that all the heat developed may be efiectively utilized. f 4

The' CSz vapor may be conducted to any suitabue condenser and cooled' to condense it into liquid form.

In the operation of thdfurnace, a pressure slightly above atmospheric is maintainedin its interior, which may be regulated simply by regulating the amount of liquid sulphur supplied to the pool'S. This prevents any infiltration of air and so excludes impurities 'which otherwise might be present. i

The conduit !5 conducts suificient heat to the charcoal passing therethrough to thoroughly dehydrate the same, driving the vapors back through the hopper !1, and thus precludes the formaticn of hydrogen sulphide in the apparatus.

While the above description refers particularly to the formation of carbon bi-sulphide, it will be apparent that it might be used for the formaticn of other compounds. For instance, by supplying chlorine and oxygen in place of the sulphur, phosgene gas may be readily generated. The heat and circulation are capable of expediting this reaction, as above described, except that it becomes unnecessary to vaporize a liquid material.

I claim:

1. The method of making carbon bi-sulphide which comprises vaporizing sulphur, raising said sulphur to a temperature above the minimum formation temperature of carbon bi-sulphide, circulating said heated vapor in a closed path, interposing carbon in said path, and continuing the circulation of the heated vapor to cause the same to repass the interposed carbon in each cycle of its circulation.

2. The method of making carbon bi-sulphide which comprises vaporizing sulphur, raising said sulphur to a temperature above the minimum ormation temperature of carbon bi-sulphide, circulating said heated vapor in a closed path, and interposing carbon in said path, continuing the circulation of the heated vapor causing the same to repass the interposed carbon in each cycle of its circulation, removing portions of the mixed sulphur vapor and carbon bi-sulphide vapor, cooling the mixed vapor below the precipitation temperature of sulphur, returning the precipitated sulphur to the atmosphere in the closed path, vaporizing the precipitated sulphur by heat from the atmosphere, and removing the un-precipitated carbon bi-sulphide vapor.

3. The method of making carbon bi-sulphide which comprises vaporizing sulphur to create an atmosphere of sulphur vapor, circulating said sulphur vapor in a closed path, interposing solid carbon in said path, continuing the circulation of the heated vapor causing the same to repass the interposed carbon in each cycle of its circulation, permitting the carbon bi-sulphide produced to circulate in vaporized condition with the vaporized sulphur, supplying heat to maintain the sulphur vapor and carbon above the minimum temperature of formation of carbon bi-sulphide, removing vapor -from one point in the closed path, cooling the removed vapor to a point below the precipitation temperature of sulphur, returning precipitated sulphur to the atmosphere circulating in the closed path, vaporizing the precipitated sulphur by heat from the atmosphere, collecting the un-precipitated carbon bi-sulphide, and supplying additional sulphur and carbon as these are consumed.

4. The continuous method of making carbon bi-sulphide which comprises melting phur and then evaporating the melted sulphur to create an atmosphere of sulphur vapor, circulating the sulphur vapor in a closed path, interposing carbon in said path, continuing the cil"- culation of the heated vapor causing the same to repass the interposed carbon in each cycle of its circulation, supplying heat suflicient to maintain the sulphur vapor and carbon above the minimum temperature of formation of carbon bi-sulphide, continuously removing vapor from one part of the closed path, cooling the removed vapor to a point below the precipitation temperature of sulphur, returning the precipitated sulphur to the circulating sulphur vapor in the closed path, permitting some of the vaporized carbon bi-sulphide to travel with the sulphur throughout the path, collecting un-precipitated carbon bi-sulphide from the vapor removed and cooled, and continusulv ously supplying additional sulphur and carbon as these materials are consumed.

5. The continuous method of producing carbon bi-sulphide which comprises circulating cyclically in a closed path an atmosphere comprising sulphur vapor and carbon bi-sulphide vapor, continuously introducing molten sulphur into contact with said circulating atmosphere, vaporizing said molten sulphur by contact with the atmosphere, supplying heat to the atmosphere in quantities capable of maintaining the temperature of said circulating atmosphere at least as high as the formation temperature of carbon bi-sulphide, dehydrating carbon, introducng the de-hydrated carbon into the path of said circulating atmosphere, permitting the formation of carbon bisulphide by contact between the carbon and the free sulphur of the circulating atmosphere, scavenging the produced carbon bi-sulphide from the surface of the carbon by means of the circulating atmosphere, continuously withdrawing some of the atmosphere from its cyclical circulating path, precipitating the free sulphur from the withdrawn atmosphere, returning the precipitated sulphur directly to the path of the circulating atmosphere, the amount of atmosphere withdrawn being suflicient to remove the carbon bi-sulphide at a rate substantially equal to its rate of formation, conveying the heat liberated by the precipitation of the sulphur, and utilizing said conveyed heat to melt solid sulphur preparatory to it introduction into contact with the circulaing atmosphere.

6. The continuous method of producing carbon bi-sulphide which comprises circulating cyclically in a closed path an atmosphere comprising sulphur vapor and carbon bi-sulphide vapor, continuously introducing molten sulphur into contact with said circulating atmosphere, vaporizing said molten sulphur by contact with the atmosphere, supplying heat to the atmosphere in quantities capable of maintaim'ng the temperature of said circulating atmosphere at least as high as the formation temperature of carbon bi-sulphide, dehydrating carbon, introducing the de-hydrated carbon into the path of said circulating atmosphere, permitting the formation of carbon bisulphide' by contact between the carbon and the free sulphur of the circulating atmosphere, scavenging the produced carbon bi-sulphide from the surface of the carbon by means of the circulating atmosphere, continuously withdrawing some of the atmosphere from its cyclical circulating path, precipitating the 'free sulphur from the withdrawn atmosphere, returning the precipitated sulphur directly to the path of the circulating atmosphere, the amount of atmosphere withdrawn being sufficient to remove the carbon bi-sulphide at a rate substantially equal to its rate of formation, conveying the heat liberated by the precipitation of the sulphur, and utilizing said conveyed heat to melt solid sulphur preparatory to its introduction into contact with the circulating atmosphere, the melted sulphur and carbon being supplied at rates substantially equal to the consumption of these materials, respectively, in the formation of carbon bi-sulphide.

FRANK H. PARSONS. 

